CN113084186A - Flower-shaped copper particle and preparation method thereof - Google Patents

Flower-shaped copper particle and preparation method thereof Download PDF

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CN113084186A
CN113084186A CN202110340778.7A CN202110340778A CN113084186A CN 113084186 A CN113084186 A CN 113084186A CN 202110340778 A CN202110340778 A CN 202110340778A CN 113084186 A CN113084186 A CN 113084186A
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shaped copper
growth substrate
copper particles
electrolyte
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CN113084186B (en
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刘晓伟
杨宝朔
刘磊
艾远
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Wuhan University WHU
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    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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    • B22F1/068Flake-like particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07Metallic powder characterised by particles having a nanoscale microstructure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
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    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/12Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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    • C25D3/00Electroplating: Baths therefor
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    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/54Electroplating of non-metallic surfaces
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Abstract

The invention provides a flower-shaped copper particle, which is 0.5-6 mu m in size and consists of 20-50 nanosheets, wherein the thickness of the nanosheets is 30-200 nm. The preparation method of the flower-shaped copper particles comprises the following steps: step S1: dissolving inorganic copper salt in distilled water, adding polyethylene glycol and saccharin as additives, and uniformly stirring to obtain electrolyte; step S2: polishing the graphite wafer, and sequentially cleaning with absolute ethyl alcohol and distilled water to obtain a growth substrate; step S3: pouring the electrolyte into an electrolytic reaction tank, respectively connecting an anode and a growth substrate with a positive electrode and a negative electrode of a direct current stabilized voltage power supply, vertically inserting the anode and the growth substrate into the electrolyte in the electrolytic reaction tank, and electrolyzing; step S4: and (4) after the electrolysis is finished, taking out the growth substrate, cleaning and drying to obtain the flower-shaped copper particles on the surface of the growth substrate. The invention finds a new method for preparing flower-shaped copper particles by using an electrodeposition method.

Description

Flower-shaped copper particle and preparation method thereof
Technical Field
The invention relates to the technical field of metal materials, in particular to a flower-shaped copper particle and a preparation method thereof.
Background
Because of excellent performances in the aspects of heat, electricity, catalysis and the like, environmental friendliness and low price, research and preparation of copper micro-nano particles increasingly attract attention of researchers, and the copper micro-nano particles are widely applied to the aspects of microelectronics, semiconductors, catalysis, batteries, bacteriostasis, sterilization and the like.
By controlling the structural characteristics and the morphological characteristics of the copper particles, the performance of the copper particles can be regulated, controlled and optimized. At present, the form of micro-nano copper particles mainly comprises: a polyhedron; sheet-shaped; a rod shape; spherical; linear shape; dendritic, etc., with less reported grain morphology. The flower-shaped particles have the characteristic of large specific surface area, have the contact area with other substances which is several times larger than that of other forms, and have more active sites and better performance in the processes of reaction, test (such as Raman scattering) and the like.
At present, the preparation method of micro-nano copper particles mainly comprises the following steps: physical chemical deposition; mechanical grinding; electro-deposition; carrying out hydrothermal reduction; ultraviolet irradiation; ultrasonic synthesis, and the like. Many methods have the problems of high requirement on environment or environmental pollution, long experimental period, many process parameters, single prepared particle form (only one type can be prepared), and the like, such as: chinese patent 201810380253.4 discloses a method for preparing free flower-shaped copper particles without a template, which successfully prepares flower-shaped copper particles, but the steps are complicated, and have special requirements (such as vacuum) on the environment, the used instruments are expensive, and only the flower shape can be prepared. Zhang wenfeng et al disclose a method for preparing flower-like nano-copper by liquid phase chemical reduction in the preparation and antibacterial properties of flower-like nano-copper, which shows excellent antibacterial and bacteriostatic properties, but the reaction period is longer, the prepared nano-copper petals are less, and the specific surface area is not increased sufficiently. The electrodeposition method is widely applied to the synthesis of copper particles as a mature preparation method, and is simple and easy to operate. Meanwhile, the micro-nano particles are easy to agglomerate in the preparation process due to high surface energy. Aiming at the problems, the invention aims to provide a flower-shaped copper particle and an electrodeposition preparation method thereof, wherein the preparation method is simple and easy to operate, has no special requirement on environment, and the prepared particle petals are rich.
Disclosure of Invention
Aiming at the problems in the background art, the invention provides a flower-shaped copper particle and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
a flower-shaped copper particle, characterized in that: the flower-shaped copper particles have the size of 0.5-6 mu m and consist of 20-50 nanosheets, and the thickness of the nanosheets is 30-200 nm.
A preparation method of flower-shaped copper particles is characterized by comprising the following steps:
step S1: dissolving inorganic copper salt in distilled water, adding polyethylene glycol and saccharin as additives, and uniformly stirring to obtain electrolyte;
step S2: polishing the graphite wafer, and sequentially cleaning with absolute ethyl alcohol and distilled water to obtain a growth substrate;
step S3: pouring the electrolyte into an electrolytic reaction tank, respectively connecting an anode and a growth substrate with a positive electrode and a negative electrode of a direct current stabilized voltage power supply, vertically inserting the anode and the growth substrate into the electrolyte in the electrolytic reaction tank, and electrolyzing;
step S4: and (4) after the electrolysis is finished, taking out the growth substrate, cleaning and drying to obtain the flower-shaped copper particles on the surface of the growth substrate.
Further, in step S1, the inorganic copper salt is one or more of copper sulfate, copper nitrate or copper chloride.
Further, the concentration of each component in the electrolyte obtained in step S1 is: cu2+In the concentration range of200 mmol/L-400 mmol/L, polyethylene glycol concentration range of 20 mmol/L-30 mmol/L, and saccharin concentration range of 0.5 g/L-1 g/L.
Further, in step S2, the mode of the grinding and polishing process is: the side surfaces of the graphite wafer were polished with 400 mesh, 1000 mesh, 2000 mesh, 4000 mesh and 10000 mesh silicon carbide sandpaper in this order, and then polished to a mirror surface.
Further, in step S2, one side surface of the graphite wafer is polished, the other side surface of the graphite wafer is insulated with a photoresist, and then washed with absolute ethyl alcohol and distilled water in sequence to obtain a growth substrate.
Further, in step S2, the graphite wafer has a diameter of 5mm to 10mm and a thickness of 2mm to 4 mm.
Further, in step S3, the electrolysis process is a constant voltage electrolysis process or a constant current electrolysis process.
Further, in step S3, during the electrolysis, the electrolysis parameters are: the voltage is 15V-20V, the current is 1A-2A, the time is 4 min-6 min, the temperature is room temperature, and the atmosphere is air.
Further, in step S3, the anode and the growth substrate are spaced apart by a distance of 4cm to 6 cm.
Further, the anode is an inert electrode or a copper electrode. The inert electrode is made of a material which does not lose electrons and does not react with the electrolyte during electrolysis, and the electrolyte contains inorganic copper salt, so that the inert electrode comprises metals (such as Pt, Au, W and the like) which are not as active as copper in a metal activity sequence table, a non-metal electrode (such as a graphite electrode) and the like; the copper electrode can supplement Cu in the electrolyte2+
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
the invention uses graphite wafer as growing base to connect power negative pole, uses polyethylene glycol and saccharin as additive, finds a new method for preparing flower-shaped copper particles by electrodeposition method, the obtained flower-shaped copper particles have higher specific surface area than other common copper particles with shape structure, and have more petals and surface area than the published flower-shaped copper particles.
Drawings
FIG. 1 is a high resolution scanning electron micrograph of flower-shaped copper particles prepared according to example 1;
FIG. 2 is a low resolution scanning electron micrograph of the flower-shaped copper particles prepared in example 1;
FIG. 3 is a high resolution scanning electron micrograph of non-flower shaped copper particles prepared according to example 3;
FIG. 4 is a low resolution scanning electron micrograph of the non-flower shaped copper particles prepared in example 3.
Detailed Description
Example 1
Step S1: dissolving inorganic copper salt in distilled water, adding polyethylene glycol and saccharin as additives, and uniformly stirring to obtain electrolyte; the concentration of each component in the electrolyte is as follows: cu2+The concentration of the saccharin is 200mmol/L, the concentration range of the polyethylene glycol is 20mmol/L, and the concentration range of the saccharin is 0.5 g/L;
step S2: grinding one side surface of the graphite wafer by using 400-mesh, 1000-mesh, 2000-mesh, 4000-mesh and 10000-mesh silicon carbide abrasive paper in sequence, then polishing the side surface to a mirror surface, performing insulation treatment on the other side surface of the graphite wafer by using a photoresist, and then cleaning by using absolute ethyl alcohol and distilled water in sequence to obtain a growth substrate; the diameter of the graphite wafer is 5mm, and the thickness of the graphite wafer is 2 mm;
step S3: pouring the electrolyte into an electrolytic reaction tank, respectively connecting an anode and a growth substrate with a positive electrode and a negative electrode of a direct current stabilized voltage power supply, vertically inserting the anode and the growth substrate into the electrolyte in the electrolytic reaction tank, and electrolyzing; the anode is a tungsten electrode; the spacing distance between the anode and the growth substrate is 4cm, the electrolysis process is a constant-voltage electrolysis process, and the electrolysis parameters are as follows: voltage 15V, current 1A, time 6min, temperature room temperature, atmosphere is air.
Step S4: and (4) after the electrolysis is finished, taking out the growth substrate, cleaning and drying to obtain the flower-shaped copper particles on the surface of the growth substrate.
Fig. 1 and 2 are high-and low-resolution scanning electron micrographs of flower-shaped copper particles prepared in example 1 of the present invention, the size of the flower-shaped copper particles being 1 to 6 μm, the thickness of the nanosheets constituting the copper particles being 50 to 200nm, each copper particle being composed of about 20 to 50 nanosheets.
Example 2
Step S1: dissolving inorganic copper salt in distilled water, adding polyethylene glycol and saccharin as additives, and uniformly stirring to obtain electrolyte; the concentration of each component in the electrolyte is as follows: cu2+The concentration range of the saccharin is 400mmol/L, the concentration range of the polyethylene glycol is 30mmol/L, and the concentration range of the saccharin is 1 g/L;
step S2: sequentially grinding two side surfaces of the graphite wafer by using 400-mesh, 1000-mesh, 2000-mesh, 4000-mesh and 10000-mesh silicon carbide abrasive paper, polishing the two side surfaces to a mirror surface, and sequentially cleaning by using absolute ethyl alcohol and distilled water to obtain a growth substrate; the diameter of the graphite wafer is 10mm, and the thickness of the graphite wafer is 4 mm;
step S3: pouring the electrolyte into an electrolytic reaction tank, respectively connecting an anode and a growth substrate with a positive electrode and a negative electrode of a direct current stabilized voltage power supply, vertically inserting the anode and the growth substrate into the electrolyte in the electrolytic reaction tank, and electrolyzing; the anode is a tungsten electrode; the spacing distance between the anode and the growth substrate is 6cm, the electrolysis process is a constant-voltage electrolysis process, and the electrolysis parameters are as follows: voltage 20V, current 2A, time 4min, temperature room temperature, atmosphere is air.
Step S4: and (4) after the electrolysis is finished, taking out the growth substrate, cleaning and drying to obtain the flower-shaped copper particles on the surface of the growth substrate.
The flower-shaped copper particles prepared in example 2 have a size of 0.5 to 6 μm, and the thickness of the nanosheets constituting the copper particles is 30 to 50nm, each copper particle being composed of about 20 to 50 nanosheets.
Example 3
Step S1: dissolving inorganic copper salt in distilled water, adding gelatin as an additive, and uniformly stirring to obtain an electrolyte; the concentration of each component in the electrolyte is as follows: cu2+The concentration range of (1) is 200mmol/L, and the concentration of the gelatin is 1 g/L;
step S2: grinding one side surface of the graphite wafer by using 400-mesh, 1000-mesh, 2000-mesh, 4000-mesh and 10000-mesh silicon carbide abrasive paper in sequence, then polishing the side surface to a mirror surface, performing insulation treatment on the other side surface of the graphite wafer by using a photoresist, and then cleaning by using absolute ethyl alcohol and distilled water in sequence to obtain a growth substrate; the diameter of the graphite wafer is 5mm, and the thickness of the graphite wafer is 2 mm;
step S3: pouring the electrolyte into an electrolytic reaction tank, respectively connecting an anode and a growth substrate with a positive electrode and a negative electrode of a direct current stabilized voltage power supply, vertically inserting the anode and the growth substrate into the electrolyte in the electrolytic reaction tank, and electrolyzing; the anode is a tungsten electrode; the spacing distance between the anode and the growth substrate is 4cm, the electrolysis process is a constant-voltage electrolysis process, and the electrolysis parameters are as follows: voltage 15V, current 1A, time 6min, temperature room temperature, atmosphere is air.
Step S4: and (4) after the electrolysis is finished, taking out the growth substrate, cleaning and drying to obtain the copper particles in the non-flower shape on the surface of the growth substrate.
FIGS. 3 and 4 are high-and low-resolution scanning electron micrographs of non-flower-shaped copper particles prepared according to example 3 of the present invention, the copper particles having a size of 400nm to 800nm, which do not exhibit flower morphology.
For the sake of non-misunderstanding, it is said that "the anode and the growth substrate are connected to the anode and the cathode of the dc regulated power supply respectively" means "the anode is connected to the anode of the dc regulated power supply, and the growth substrate is connected to the cathode of the dc regulated power supply".
The experiments of the embodiment 1 and the embodiment 2 show that the graphite wafer is used as a growth substrate, connected with a power supply negative electrode, and electrolyzed by using polyethylene glycol and saccharin as additives, so that flower-shaped copper particles can grow, the size of the flower-shaped copper particles is 0.5-6 μm, the flower-shaped copper particles are composed of 20-50 nanosheets, and the thickness of the nanosheets is 30-200 nm. Example 3 as a comparative example to example 1, it differs from example 1 only in that example 3 uses gelatin as an additive, whereas the electrodeposited product is a non-flower-shaped copper particle.

Claims (10)

1. A flower-shaped copper particle, characterized in that: the flower-shaped copper particles have the size of 0.5-6 mu m and consist of 20-50 nanosheets, and the thickness of the nanosheets is 30-200 nm.
2. A method for producing flower-shaped copper particles according to claim 1, comprising the steps of:
step S1: dissolving inorganic copper salt in distilled water, adding polyethylene glycol and saccharin as additives, and uniformly stirring to obtain electrolyte;
step S2: polishing the graphite wafer, and sequentially cleaning with absolute ethyl alcohol and distilled water to obtain a growth substrate;
step S3: pouring the electrolyte into an electrolytic reaction tank, respectively connecting an anode and a growth substrate with a positive electrode and a negative electrode of a direct current stabilized voltage power supply, vertically inserting the anode and the growth substrate into the electrolyte in the electrolytic reaction tank, and electrolyzing;
step S4: and (4) after the electrolysis is finished, taking out the growth substrate, cleaning and drying to obtain the flower-shaped copper particles on the surface of the growth substrate.
3. The method for preparing flower-shaped copper particles according to claim 2, wherein in step S1, the inorganic copper salt is one or more of copper sulfate, copper nitrate or copper chloride.
4. The method for producing flower-shaped copper particles according to claim 2, wherein the electrolyte obtained in step S1 contains the following components in concentrations: cu2+The concentration range of the saccharin is 200 mmol/L-400 mmol/L, the concentration range of the polyethylene glycol is 20 mmol/L-30 mmol/L, and the concentration range of the saccharin is 0.5 g/L-1 g/L.
5. The method for producing flower-shaped copper particles according to claim 2, wherein in step S2, the polishing process is performed by: the side surfaces of the graphite wafer were polished with 400 mesh, 1000 mesh, 2000 mesh, 4000 mesh and 10000 mesh silicon carbide sandpaper in this order, and then polished to a mirror surface.
6. The method for producing flower-shaped copper particles as claimed in claim 2, wherein in step S2, one side surface of the graphite wafer is subjected to a grinding and polishing treatment, the other side surface of the graphite wafer is subjected to an insulating treatment with a photoresist, and thereafter, the wafer is washed with absolute ethyl alcohol and distilled water in this order to obtain a growth substrate.
7. The method for producing flower-shaped copper particles according to claim 2, wherein in step S2, the graphite wafer has a diameter of 5mm to 10mm and a thickness of 2mm to 4 mm.
8. The method for producing flower-shaped copper particles according to claim 2, wherein in step S3, the electrolysis process is a constant-voltage electrolysis process or a constant-current electrolysis process.
9. The method for producing flower-shaped copper particles according to claim 2, wherein in step S3, the electrolysis parameters during electrolysis are: the voltage is 15V-20V, the current is 1A-2A, the time is 4 min-6 min, the temperature is room temperature, and the atmosphere is air.
10. The method for producing flower-shaped copper particles according to claim 2, wherein the anode is spaced apart from the growth substrate by a distance of 4cm to 6cm in step S3.
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常文贵等: "电化学法制备纳米铜粒子", 《皖西学院学报》 *

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